Preparation method for p-benzoquionone dioxime

A technology of p-benzoquinone dioxime and phenol, which is applied in the field of organic synthesis, can solve the problems of high cost and low yield, and achieve the effect of increasing yield and reducing cost

Inactive Publication Date: 2008-03-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method yield is low (about 60%), and strong base is used as solvent, so that strong base-resistant and strong-acid equipment is needed during mass production, and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] The first step is to dissolve 11.4g of sodium nitrite in 50ml of water, cool to 5°C for later use, add 10.4g of phenol into the reactor, inject sodium nitrite, ice bath, slowly add acetic acid with a mass fraction of 30% under stirring 20g, then add dropwise 39.2g of sulfuric acid with a mass fraction of 40% that has been ice-bathed in advance within 40min, (phenol, sodium nitrite, acetic acid molar ratio 1:1.5:0.33) after the dropwise addition, keep 0°C and stir evenly for 1 hour . At this time, a large number of pale yellow crystals were precipitated.

[0012] In the second step, the reaction product of the first step is suction-filtered, washed with a small amount of water, and prepared with a mass fraction of 35% hydroxylamine chloride solution 21.8g (the ratio of the amount of hydroxylamine chloride to phenol is 1.1: 1), adding the first In the step product, stir evenly. Oxime at 70°C for 3 hours, then filter the product with suction, wash with water, and dry to ...

Embodiment 2

[0014] The first step is to dissolve 11.4g of sodium nitrite in 50ml of water, cool to 5°C for later use, add 10.4g of phenol into the reactor, inject sodium nitrite, ice bath, slowly add acetic acid with a mass fraction of 30% under stirring 20g, then add dropwise 39.2g of sulfuric acid with a mass fraction of 40% that has been ice-bathed in advance within 40min, (phenol, sodium nitrite, acetic acid molar ratio 1:1.5:0.33) after the dropwise addition, keep 0°C and stir evenly for 1 hour . At this time, a large number of pale yellow crystals were precipitated.

[0015] In the second step, the reaction product of the first step is suction-filtered, washed with a small amount of water, and prepared with a mass fraction of 35% hydroxylamine chloride solution 25.8g (the ratio of the mass of hydroxylamine chloride to phenol is 1.3: 1), adding the first In the step product, stir evenly. Oxime at 70°C for 3 hours, then filter the product with suction, wash with water, and dry to ob...

Embodiment 3

[0017] The first step is to dissolve 11.4g of sodium nitrite in 50ml of water, cool to 5°C for later use, add 10.4g of phenol into the reactor, inject sodium nitrite, ice bath, slowly add acetic acid with a mass fraction of 30% under stirring 20g, then add dropwise 39.2g of sulfuric acid with a mass fraction of 40% that has been ice-bathed in advance within 40min, (phenol, sodium nitrite, acetic acid molar ratio 1:1.5:0.33) after the dropwise addition, keep 0°C and stir evenly for 1 hour . At this time, a large number of pale yellow crystals were precipitated.

[0018] In the second step, the reaction product of the first step is suction-filtered, washed with a small amount of water, and prepared with a mass fraction of 31.7 g of hydroxylamine chloride solution (the ratio of hydroxylamine chloride to phenol is 1.6: 1), and the first In the step product, stir evenly. Oxime at 70°C for 3 hours, then filter the product with suction, wash with water, and dry to obtain 11.9 g of ...

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PUM

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Abstract

The present invention relates to catalytic synthesis process of p-benzoquinone dioxime, belongs to the field of organic synthesis technology, and is especially catalytic synthesis process of p-benzoquinone dioxime through nitrosating phenol with acetic acid as catalyst. The technological scheme of the present invention adopts phenol, sodium nitrite, sulfuric acid, acetic acid and hydroxylamine chloride as materials. Phenol, sodium nitrite and acetic acid mixture are first nitrosation reacted; and through the subsequent washing with small amount of water, and adding hydroxylamine chloride for oximation, p-benzoquinone dioxime product is obtained. The process has mild reaction condition, low cost and high p-benzoquinone dioxime yield.

Description

technical field [0001] The present invention relates to a method for catalytically synthesizing p-benzoquinone dioxime, to be exact, a method for synthesizing p-benzoquinone dioxime by catalyzing nitrosation of phenol with acetic acid, belonging to the technical field of organic synthesis. Background technique [0002] P-benzoquinone dioxime is a cross-linking agent, which has the characteristics of easy dispersion in the rubber compound, fast vulcanization speed, high tensile strength of the rubber compound, heat resistance, ozone resistance, and good electrical insulation. It can be used as a polymerization inhibitor for acrylic acid agent, metallic glass hot-melt adhesive, olefin copolymer crosslinking regulator, organic monomer stabilizer and self-vulcanizing adhesive. Oxidants (Pb 3 o 4 , PbO 2 ) has an activation effect and improves the thermal resistance of polyester fiber tire cords [cf.: GogotovA.F., Parilova M.V., Amosov V.V., Khaliullin A.K. (OAO "angarskaya Ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/46C07C249/04
Inventor 单永奎贺峥孔爱国王海文施沈一
Owner EAST CHINA NORMAL UNIV
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